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采用超声化学法,以 1-甲基-2-吡咯烷酮为溶剂,简便合成 MOF-177。

Facile synthesis of MOF-177 by a sonochemical method using 1-methyl-2-pyrrolidinone as a solvent.

机构信息

Department of Chemical Engineering, Inha University, Incheon, Korea 402-751.

出版信息

Dalton Trans. 2010 Mar 21;39(11):2883-7. doi: 10.1039/b925088c. Epub 2010 Feb 5.

Abstract

High quality MOF-177 crystals in the size range of 5-20 microm were successfully synthesized via a sonochemical route in a substantially reduced synthesis time (40 min) in the presence of low-cost NMP (1-methyl-2-pyrrolidone) as a solvent. Microwave heating in NMP also produced MOF-177 under similar conditions (35 min, 5-50 microm) but exhibited inferior crystallinity. In comparison, a conventional solvothermal route in DEF (diethylformamide) took 48 h to produce MOF-177 crystals 0.5-1.5 mm in size. The BET surface areas of the MOF-177 samples decreased in the order of sonochemical (4898 m(2) g(-1)) > conventional (4833 m(2) g(-1)) > microwave route (4197 m(2) g(-1)). In line with this trend, MOF-177 prepared via the sonochemical route resulted in the highest CO(2) adsorption capacity, 1315 mg g(-1) at 30 bar and 298 K. The product yield of MOF-177 synthesized via the sonochemical route was 95.6%, and was significantly higher than the product yields of other methods.

摘要

通过超声化学途径,在 NMP(N-甲基-2-吡咯烷酮)作为溶剂的情况下,成功地在大大缩短的合成时间(40 分钟)内合成了尺寸范围在 5-20 微米的高质量 MOF-177 晶体。微波加热在 NMP 下也能在类似条件下(35 分钟,5-50 微米)产生 MOF-177,但结晶度较差。相比之下,在 DEF(二乙基甲酰胺)中的常规溶剂热途径需要 48 小时才能产生 0.5-1.5 毫米大小的 MOF-177 晶体。MOF-177 样品的 BET 表面积按超声化学途径(4898 m(2) g(-1))>常规途径(4833 m(2) g(-1))>微波途径(4197 m(2) g(-1))的顺序递减。与此趋势一致,通过超声化学途径制备的 MOF-177 具有最高的 CO(2)吸附容量,在 30 巴和 298 K 时为 1315 mg g(-1)。通过超声化学途径合成的 MOF-177 的产物产率为 95.6%,明显高于其他方法的产物产率。

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